5-(1-Methyl-3,4,5,6,7,7-hexachloro-norborn-4-ene-1)-isophthalic acid
    5.
    发明授权
    5-(1-Methyl-3,4,5,6,7,7-hexachloro-norborn-4-ene-1)-isophthalic acid 失效
    5-(1-甲基-3,4,5,6,7,7-六氯 - 降冰片-4-烯-1) - 间苯二甲酸

    公开(公告)号:US3903144A

    公开(公告)日:1975-09-02

    申请号:US40248673

    申请日:1973-10-01

    摘要: New chemical compounds useful as intermediates are 5-(1-methyl3,4,5,6,7,7-hexahalo-norborn-4-ene-1)-isophthalic acid and 4-(1methyl-3,4,5,6,7,7-hexaholo-norborn-4-ene-1)-orthophthalic acid, formed by oxidation of the primary or secondary alkyl groups containing from one to ten carbon atoms on the benzene ring of the Diels-Alder adduct of equimolecular amounts of hexahalocyclopentadiene and either 3,5-dialkyl- Alpha -methylstyrene and 3,4-dialkyl- Alpha -methylstyrene. The acyl derivatives of these intermediates do not burn or support combustion and are also useful as extreme-pressure additives in lubricating oils. The following acyl derivatives of 5-(1-methyl3,4,5,6,7,7-hexachloro-norborn-4-ene-1)-isophthalic acid have been prepared: the dichloride, diamide, dianilide, diethylester, polyphenylester, poly(chlorophenyl) ester, poly-ethylene glycol ester, diphenylthioester, di-methallylester, and unsaturated polyester. Also, the co-polyphenylesters of 5-(1-methyl3,4,5,6,7,7-hexachloro-norborn-4-ene-1)- isophthalic acid and terephthalic or adipic acid; the polyamide of 5-(1-methyl3,4,5,6,7,7-hexachloro-norborn-4-ene-1)-isophthalic acid and 1,6hexanediamine; the copolyamides of 5-(1-methyl-3,4,5,6,7,7hexachloronorborn-4-ene-1) isophthalic acid and 1,6-hexanediamine and terephthalic acid or adipic acid; the co-polyethylene glycol ester of 5-(1-methyl-3,4,5,6,7,7-hexachloro-norborn-4-ene-1) isophthalic acid and terephthalic acid; and a phosphorus adduct of 5-(1-methyl-3,4,5,6,7,7- hexachloro-norborn-4-ene-1) have been prepared.

    摘要翻译: 可用作中间体的新化合物是5-(1-甲基-3,4,5,6,7,7-六氢降冰片-4-烯-1) - 间苯二甲酸和4-(1-甲基-3,4 ,5,6,7,7-六氢降冰片-4-烯-1) - 邻苯二甲酸,其通过在Diels-Alder加合物的苯环上氧化含有1至10个碳原子的伯或仲烷基而形成 的等摩尔量的六氢环戊二烯和3,5-二烷基-α-甲基 - 苯乙烯和3,4-二烷基-α-甲基苯乙烯。 这些中间体的酰基衍生物不燃烧或支持燃烧,也可用作润滑油中的极压添加剂。 制备了以下5-(1-甲基-3,4,5,6,7,7-六氯 - 降冰片-4-烯-1) - 间苯二甲酸的酰基衍生物:二氯化物,二酰胺,二酰苯胺,二乙酯, 聚苯基酯,聚(氯苯基)酯,聚乙二醇酯,二苯硫酯,二 - 甲代烯丙基酯和不饱和聚酯。 此外,5-(1-甲基-3,4,5,6,7,7-六氯 - 降冰片-4-烯-1) - 间苯二甲酸和对苯二甲酸或己二酸的共聚苯酯; 5-(1-甲基-3,4,5,6,7,7-六氯 - 降冰片-4-烯-1) - 间苯二甲酸和1,6-己二胺的聚酰胺; 5-(1-甲基-3,4,5,6,7,7-六氯乙烯-4-烯-1)间苯二甲酸和1,6-己二胺和对苯二甲酸或己二酸的共聚酰胺; 5-(1-甲基-3,4,5,6,7,7-六氯 - 降冰片-4-烯-1)间苯二甲酸和对苯二甲酸的共聚乙二醇酯; 并制备了5-(1-甲基-3,4,5,6,7,7-六氯 - 降冰片-4-烯-1)的磷加成物。

    Continuous slurry process for formation of aromatic polycarboxylic acids
    7.
    发明授权
    Continuous slurry process for formation of aromatic polycarboxylic acids 失效
    用于形成芳族多元羧酸的连续浆料方法

    公开(公告)号:US3873609A

    公开(公告)日:1975-03-25

    申请号:US32152373

    申请日:1973-01-05

    摘要: The solid-state disproportionation of potassium benzoate to dipotassium terephthalate and benzene using zinc benzoate catalyst is conducted with the solid reagents dispersed as a slurry in liquid terphenyl diluent. The reactor effluent is water-quenched to obtain a liquid terphenyl phase, a water phase containing dissolved phthalates, and solid spent zinc oxide catalyst. The catalyst is separated by filtration, reslurried in terphenyl, reacted with benzoic acid to regenerate zinc benzoate, and the resultant catalyst slurry recycled to the reactor. The solids-free aqueous phase is contacted with benzoic acid to precipitate terephthalic acid crystals and form soluble potassium benzoate. The crystals are separated by filtration and recovered as a product of the process. The aqueous potassium benzoate solution is concentrated by evaporation and then contacted with hot terphenyl to produce a slurry of solid potassium benzoate in terphenyl for recycle to the reactor. Byproduct benzene is vented from the reactor and/or the effluent quench step.

    摘要翻译: 使用苯甲酸锌催化剂,苯甲酸钾对苯二甲酸二钾和苯的固态歧化用固体试剂作为浆液分散在液体三联苯稀释剂中进行。 将反应器流出物水淬,得到液体三联苯相,含有溶解的邻苯二甲酸酯的水相和固体废氧化锌催化剂。 通过过滤分离催化剂,在三联苯中重新成型,与苯甲酸反应以再生苯甲酸锌,并将所得催化剂浆料再循环至反应器。 不含固体的水相与苯甲酸接触以析出对苯二甲酸晶体并形成可溶的苯甲酸钾。 通过过滤分离晶体并作为该方法的产物回收。 通过蒸发浓缩含水的苯甲酸钾溶液,然后与热三联苯接触,产生固体苯甲酸钾在三联苯中的浆液循环到反应器中。 副产物苯从反应器和/或流出物骤冷步骤排出。